You are on page 1of 7

INTRODUCTION

The purpose of this lab is to separate Methanol and Water from a binary Methanol/Water
mixture. The two components are mixed and fed into the column and readings are taken at
different stages to see what the concentrations are. A calibration curve is set up using known
values of Methanol and Water and these samples are compared against the known value on the
curve. When the column reaches steady state the finals readings are taken for the distillate and
the bottoms stream. Distillation works by using the boiling point differences of the components.
As the mixture is heated up the majority of the light key component (the component with the
lower boiling point) goes into the vapor state. As this comes into contact with the liquid coming
down on the same stage the concentration of the vapor goes up in the light key component and at
the same time the concentration of the heavy key (the component with a higher boiling point)
goes up in the liquid state.

Distillation columns typically have several stages where the vapor and liquid streams
come into contact and each stream gets concentrated in the respective light and heavy key
components. There is a re-boiler on the bottom that boils the liquid falling down the stages due to
gravity. This boiled up liquid travels up the stages and carries the light key component with it.
There is also a condenser at the top of the column, most of the vapor that goes up gets condensed
and it repeats the cycle of going down the column, boil, and come back up. The product coming
out of the top is called the distillate it’s the stream that is concentrated in the light key
component, for this lab this stream will contain mostly Methanol since the boiling point of
Methanol is lower than that of water. The product coming out of the bottom is called the bottoms
product and for this lab water will consist mostly of the bottoms stream.

5. Else. maintain the tank with alcohol to conduct further experiments. . 9. 7. 2. The inlet hose is attached from the condenser unit to a cold water supply and the outlet hose to a drain. Turn off the water supply and disconnect the hoses if not required. drain off the contents in the reboiler with valves (DV01). as long as they are uncontaminated. reflux tank (DV02) and top product tank (DV106). Attach the inlet hose from the condenser unit to a cold water supply and the outlet hose to a drain. Switch off the main power unit and power supply. The unit is connected to a 415 VAC 3 phase 50 Hz power supply and the power supply is switched on. Switch ON the main power switch in front of both of the control panels on the unit. The unit is now ready for experiments. Connect the unit to a 415 VAC 3 phase 50 Hz power supply and switch on the power supply. Ensure that all valves on the unit are closed. Open valves V105 and V107 for initial vacuum suction application if desired. close V105 and V107 when the vacuum pressure reaches 0. For storage purposes during a long break. Do not open the reboiler cap while the contents are at high temperatures as vapors might rush out of the tank. After the experiment. leave the sieve plate column for 20 minutes to cool down. 4. 3.2 bar. 6. EXPERIMENT PRE-PROCEDURE 1. All alcohol samples can be re-used after the experiment. 8. All hand valves on the unit are ensured to be closed except the one on the water inlet valve V104.PROCEDURE General Start-up Procedures 1. Keep an eye on the pressure gauge. 2.

Valve V106 on the Top product tank is opened. 50% volume ethanol is recommended in water mixture 2. Valves V105 and V107 is opened if initial vacuum suction is required. the column leaved at total reflux (100%) for another 5 minutes to allow the system to stabilize. 12. Valve V104 is opened. The main power switches is switched on the unit. All the valves on this unit is closed. The pressure gauge. Note: please take note of the temperature change on T11. 6. The Reboiler heater ON/OFF switch is switched on located on the Control Panel. The reflux controller indicates percentage of condensate returning to the column. 10 mL of the prepared sample is collected using a syringe and test the refractive index. T15 to 88ºC by pressing UP or DOWN button. Whenop product appears in the divider vessel. 5. The vapor to condense is condened in the glass condenser. 3. 13. it will begin to show condensate collection. Note: high power setting is required in order to supply sufficient energy to warm the system up in the initial startup. 9. NOTE: Do not open valves V105 and V107 when the experiment is running. .2 bar. The mixture is poured into the reboiler as shown in the picture. when T11 reaches about 80ºC. Cooling water supply is started. 10.PROCEDURE (CONSTANT REFLUX) 1. 11. The reflux switch is on and reflux is set to 100%. 8. close V105 and V107 was carefully monitored when the vacuum pressure reaches 0. 10 L batch of binary mixture (refer to chemical preparation) of known composition is prepared. 4. Temperature of reboiler is set from. 7. The power of the boiler is set to maximum using the power regulator.

The mixture is poured into the reboiler as shown in picture 1 in page 23. close V105 and V107 was carefully monitored when the vacuum pressure reaches 0.the top product is emptied in the vessel and its volume is measured. The reboiler’s sample. 15. 10 mL of the prepared sample is collected using a syringe and test the refractive index. glasses. 17. 14. as long as they are uncontaminated. Valves V105 and V107 is opened if initial vacuum suction is required. laboratory cloth. The main power switches is switched on the unit. 18. The pressure gauge. Note: you are recommended to wear protective gloves. . 6 set of readings is taken. Then . The refractive index of each sample is measured at constant room temperatures. 16. 4. All the data as shown is tabulated in table. PROCEDURE (REGULATING REFLUX) 1. long pants and covered shoes when taking samples from top product (DV03) and reboiler tank (DV01). 19. 50% volume ethanol is recommended in water mixture 2. is quickly cooled down and the sample tube placed in a beaker filled with cold water. At every intervals of 5 minutes. This will give us the product output rate of the system. Reflux control is changed to a desired value i. NOTE: Do not open valves V105 and V107 when the experiment is running.e. 7. 10 L batch of binary mixture (refer to chemical preparation) of known composition is prepared. all temperatures is recorded and small sample (approximately 10ml) is draw from the top product tank (DV03) and reboiler tank (DV01). Cooling water supply is started. All alcohol samples have be re-used after the experiment. All the temperatures iw recorded as the initial experiment point. Valve V104 is opened. All the valves on this unit is closed. 6. 3.2 bar. 5. 80%.

laboratory cloth. Then. The reflux switch is on and reflux is set to 100%. 16. Note: please take note of the temperature change on T11. . glasses. All the temperatures iw recorded as the initial experiment point. All alcohol samples have be re-used after the experiment. Reflux ratio changed to 30% and then changed to a desired value of. This will give us the product output rate of the system. Valve V106 on the Top product tank is opened. The reflux controller indicates percentage of condensate returning to the column. 18. Note: you are recommended to wear protective gloves. 10. 12. 13. the column leaved at total reflux (100%) for another 5 minutes to allow the system to stabilize. all temperatures is recorded and small sample (approximately 10ml) is drawed from the top product tank (DV03) and reboiler tank (DV01). The refractive index of each sample is measured at constant room temperatures. the top product is emptied in the vessel and its volume is measured.8. 17. it will begin to show condensate collection. when T11 reaches about 80ºC. 11. The vapor to condense is condened in the glass condenser. long pants and covered shoes when taking samples from top product (DV03) and reboiler tank (DV01). 80%. as long as they are uncontaminated. 14. Whenop product appears in the divider vessel. Temperature of reboiler is set from. The Reboiler heater ON/OFF switch is switched on located on the Control Panel. 15. 9. The power of the boiler is set to maximum using the power regulator. Note: high power setting is required in order to supply sufficient energy to warm the system up in the initial startup. At every intervals of 5 minutes. All the data as shown is tabulated in table. T15 to 88ºC by pressing UP or DOWN button. 6 set of readings is taken. The reboiler’s sample. 19. is quickly cooled down and the sample tube placed in a beaker filled with cold water.

Reflux Divider G .Reboiler / Evaporator B .Reflux Valve J .Top product tank L . Figure shows the distillation column used for the experiment A .Control Panel .Distillation column C .Sampling ports D .Condenser F .Water jet vacuum K .Differential Pressure Gauge E .